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Preparation method of immobilized alkaline ionic liquid catalyst

A liquid catalyst, basic ion technology, applied in physical/chemical process catalysts, chemical instruments and methods, organic compound/hydride/coordination complex catalysts, etc., can solve the problem of high cost, low catalyst activity, difficult recovery, etc. problem, to achieve the effect of reducing preparation cost, high catalyst activity, and no pollution

Active Publication Date: 2013-11-27
灯塔森佳新能源合伙企业(有限合伙)
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0011] The technical problem to be solved in the present invention is aimed at the defects of low catalyst activity, difficult recovery and high cost in the transesterification reaction of current ionic liquid catalysts.

Method used

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  • Preparation method of immobilized alkaline ionic liquid catalyst
  • Preparation method of immobilized alkaline ionic liquid catalyst
  • Preparation method of immobilized alkaline ionic liquid catalyst

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] (1) Add toluene, pure silicon molecular sieve MCM-41 and chloroacetyl chloride in sequence in a round bottom flask, wherein the mass ratio of pure silicon molecular sieve MCM-41 to toluene is 1:30, pure silicon molecular sieve MCM-41 and chloroacetyl chloride The mass ratio is 8:1. Magnetically stirred and reacted at -10°C for 6 hours to obtain pure silicon molecular sieves with esterified hydroxyl groups on the surface.

[0028] (2) After filtering, washing and drying the reaction system obtained in step (1), put the obtained solid into a dry round bottom flask, and then add toluene and 1-methylimidazole in sequence, wherein the mass of toluene and solid The ratio is 10:1, the mass ratio of 1-methylimidazole to solid is 0.2:1, heated to 60°C with magnetic stirring for 6 hours, and the immobilized ionic liquid with pure silicon molecular sieve as carrier can be obtained.

[0029] (3) Add the immobilized ionic liquid obtained in step (2) into a round-bottomed flask, and...

Embodiment 2

[0031] (1) Add toluene, pure silicon molecular sieve MCM-48 and chloroacetyl chloride in sequence in a round bottom flask, wherein the mass ratio of pure silicon molecular sieve MCM-48 to toluene is 1:30, pure silicon molecular sieve MCM-48 and chloroacetyl chloride The mass ratio is 8:1. The reaction was carried out under magnetic stirring at 30° C. for 6 hours to obtain a pure silicon molecular sieve with esterified hydroxyl groups on the surface.

[0032] (2) After filtering, washing and drying the reaction system obtained in step (1), add the obtained solid into a round bottom flask, and then add toluene and 1-methylimidazole in sequence, wherein the mass ratio of toluene to solid is 10 : 1, The mass ratio of 1-ethylimidazole to solid is 0.5:1, heated to 100° C. for 6 hours with magnetic stirring, and the immobilized ionic liquid with pure silicon molecular sieve as carrier can be obtained.

[0033] (3) Add the immobilized ionic liquid obtained in step (2) into a round bo...

Embodiment 3

[0035] (1) Add toluene, pure silicon molecular sieve SBA-15 and chloroacetyl chloride in sequence in a round bottom flask, wherein the mass ratio of pure silicon molecular sieve SBA-15 to toluene is 1:30, pure silicon molecular sieve SBA-15 and chloroacetyl chloride The mass ratio is 8:1. The reaction was carried out under magnetic stirring at 10° C. for 6 hours to obtain pure silicon molecular sieves with esterified hydroxyl groups on the surface.

[0036] (2) After filtering, washing and drying the reaction system obtained in step (1), add the obtained solid into a round bottom flask, and then add toluene and 1-propylimidazole in sequence, wherein the mass ratio of toluene to solid is 10 : 1, The mass ratio of 1-propylimidazole to solid is 0.3:1, and heated to 100° C. for 6 hours with magnetic stirring to obtain an immobilized ionic liquid with pure silicon molecular sieve as the carrier.

[0037] (3) Add the immobilized ionic liquid obtained in step (2) into a round bottom...

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Abstract

The invention relates to a preparation method of an immobilized alkaline ionic liquid catalyst for ester exchange reaction. According to the method, by using pure silicon molecular sieves or silicon dioxide microbeads as a support and chloracetyl chloride, 1-alkyliminazole and tetramethylammonium hydroxide as raw materials, the ionic liquid can be effectively immobilized on the surface of the pure silicon molecular sieves or silicon dioxide microbeads by three reaction steps. The method is simple; and the obtained immobilized alkaline ionic liquid catalyst after reaction can be recycled for cyclic utilization after simple treatment, and thus, has the advantages of long service life and no pollution, thereby greatly lowering the reaction cost. The catalyst has favorable effect when being used in the ester exchange reaction of synthesizing methylethyl carbonate from dimethyl carbonate and diethyl carbonate.

Description

technical field [0001] The invention relates to the field of preparation of immobilized alkaline ionic liquids, in particular to a method for preparing an immobilized alkaline ionic liquid catalyst used for transesterification. Background technique [0002] At present, most of the catalysts used in the transesterification reaction are alkaline, such as NaOH, KOH, NaOCH 3 、KOCH 3 etc., these catalysts have high activity, but in the actual application process, it is found that this type of catalyst has poor solubility in the reaction solution, is easy to precipitate, and is easy to foul. Precipitation in the medium, clogging the pipeline. Moreover, these catalysts are difficult to separate from the product, which prompts people to study highly active and easy-to-separate heterogeneous catalysts. [0003] Several heterogeneous catalysts have been reported in the literature, such as quaternary ammonium type strong base resin, sulfonic acid type strong acid resin, carboxylic a...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J31/02C07C69/96C07C68/06
Inventor 薛冰郭静周校蕾李永昕柳娜许杰
Owner 灯塔森佳新能源合伙企业(有限合伙)
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